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#$Date: 2021-02-03 12:19:03 +0200 (Wed, 03 Feb 2021) $
#$Revision: 261393 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/02/1560258.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1560258
loop_
_publ_author_name
'Najla Mahbouli Rhouma'
'Ali Rayes'
'Francesco Mezzadri'
'Davide Delmonte'
'Riccardi Cabassi'
'Gianluca Calestani'
'Mohamed Loukil'
_publ_section_title
;
 Structural and electrical phase transitions in the
 [(C2H5)4N]2ZnI3.86Cl0.14 system
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              60
_journal_page_last               66
_journal_paper_doi               10.1016/j.jssc.2017.08.029
_journal_volume                  256
_journal_year                    2017
_chemical_formula_moiety         '2(C8 H20 N), Cl0.12 I3.88 Zn'
_chemical_formula_sum            'C16 H40 Cl0.12 I3.88 N2 Zn'
_chemical_formula_weight         822.15
_chemical_name_common
;
2(C8 H20 N), Cl0.12 I3.88 Zn
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7327(8)
_cell_length_b                   13.7327(8)
_cell_length_c                   14.7484(8)
_cell_measurement_reflns_used    213
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      18.02
_cell_measurement_theta_min      8.60
_cell_volume                     2781.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX2 CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31860
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.489
_diffrn_reflns_theta_min         1.381
_exptl_absorpt_coefficient_mu    5.158
_exptl_absorpt_correction_T_max  0.233
_exptl_absorpt_correction_T_min  0.156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2772
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0312P)²+3.4713P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2668
_reflns_number_total             2772
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            JSSC-2017-256-60-2.cif
_cod_data_source_block           O_233
_cod_original_cell_volume        2781.4(4)
_cod_database_code               1560258
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.245
_shelx_estimated_absorpt_t_max   0.326
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.75234(7) 0.25234(7) 0.22828(8) 0.0518(4) Uani 1 2 d S T P . .
I1 I 0.62954(5) 0.12954(5) 0.29921(6) 0.0680(3) Uani 0.969(7) 2 d S T P . .
I2 I 0.74487(5) 0.24487(5) 0.05220(5) 0.0614(2) Uani 0.969(7) 2 d S T P . .
I3 I 0.70412(5) 0.42756(4) 0.28002(4) 0.0757(2) Uani 0.969(7) 1 d . . P . .
Cl1 Cl 0.62954(5) 0.12954(5) 0.29921(6) 0.0680(3) Uani 0.031(7) 2 d S T P . .
Cl2 Cl 0.74487(5) 0.24487(5) 0.05220(5) 0.0614(2) Uani 0.031(7) 2 d S T P . .
Cl3 Cl 0.70412(5) 0.42756(4) 0.28002(4) 0.0757(2) Uani 0.031(7) 1 d . . P . .
N1 N 0.7904(5) 0.2904(5) 0.5794(6) 0.053(2) Uani 1 2 d DS T P . .
N2 N 0.5000 0.5000 0.0000 0.047(3) Uani 1 4 d DS T P . .
N3 N 0.5000 0.0000 -0.0145(9) 0.062(4) Uani 1 4 d DS T P . .
C1 C 0.7165(7) 0.2165(7) 0.5491(12) 0.092(5) Uani 1 2 d DS T P . .
H1A H 0.7497 0.1683 0.5110 0.111 Uiso 0.5 1 calc R U P . .
H1B H 0.6683 0.2497 0.5110 0.111 Uiso 0.5 1 calc R U P . .
C2 C 0.6625(9) 0.1625(9) 0.6238(15) 0.119(7) Uani 1 2 d DS TU P . .
H2A H 0.7010 0.1072 0.6434 0.179 Uiso 0.5 1 calc R U P . .
H2B H 0.6003 0.1400 0.6009 0.179 Uiso 0.5 1 calc R U P . .
H2C H 0.6520 0.2060 0.6746 0.179 Uiso 0.5 1 calc R U P . .
C3 C 0.8326(7) 0.3326(7) 0.4951(9) 0.083(4) Uani 1 2 d DS TU P . .
H3A H 0.7796 0.3609 0.4593 0.099 Uiso 0.5 1 calc R U P . .
H3B H 0.8609 0.2796 0.4593 0.099 Uiso 0.5 1 calc R U P . .
C4 C 0.9088(7) 0.4088(7) 0.5087(12) 0.101(5) Uani 1 2 d DS TU P . .
H4A H 0.8778 0.4710 0.5206 0.151 Uiso 0.5 1 calc R U P . .
H4B H 0.9485 0.4138 0.4544 0.151 Uiso 0.5 1 calc R U P . .
H4C H 0.9496 0.3911 0.5597 0.151 Uiso 0.5 1 calc R U P . .
C5 C 0.8674(8) 0.2433(9) 0.6361(6) 0.085(3) Uani 1 1 d D U . . .
H5A H 0.8367 0.2155 0.6902 0.102 Uiso 1 1 calc R U . . .
H5B H 0.9132 0.2935 0.6563 0.102 Uiso 1 1 calc R U . . .
C6 C 0.9247(9) 0.1628(9) 0.5875(9) 0.102(4) Uani 1 1 d D U . . .
H6A H 0.8809 0.1100 0.5717 0.152 Uiso 1 1 calc R U . . .
H6B H 0.9754 0.1385 0.6273 0.152 Uiso 1 1 calc R U . . .
H6C H 0.9540 0.1890 0.5329 0.152 Uiso 1 1 calc R U . . .
C7 C 0.4619(7) 0.5820(7) -0.0578(7) 0.072(3) Uani 1 1 d D . . . .
H7A H 0.5165 0.6113 -0.0908 0.087 Uiso 1 1 calc R U . . .
H7B H 0.4344 0.6322 -0.0182 0.087 Uiso 1 1 calc R U . . .
C8 C 0.3836(7) 0.5503(9) -0.1267(6) 0.079(3) Uani 1 1 d D . . . .
H8A H 0.4097 0.4995 -0.1654 0.119 Uiso 1 1 calc R U . . .
H8B H 0.3648 0.6058 -0.1635 0.119 Uiso 1 1 calc R U . . .
H8C H 0.3271 0.5258 -0.0945 0.119 Uiso 1 1 calc R U . . .
C9 C 0.5139(18) 0.0895(15) -0.0690(15) 0.103(8) Uani 0.5 1 d D . P A -1
H9A H 0.5263 0.1435 -0.0272 0.123 Uiso 0.5 1 calc R U P A -1
H9B H 0.4526 0.1035 -0.1003 0.123 Uiso 0.5 1 calc R U P A -1
C10 C 0.595(3) 0.089(4) -0.1395(15) 0.151(10) Uani 0.5 1 d D U P A -1
H10A H 0.5962 0.1509 -0.1709 0.227 Uiso 0.5 1 calc R U P A -1
H10B H 0.5833 0.0370 -0.1829 0.227 Uiso 0.5 1 calc R U P A -1
H10C H 0.6570 0.0782 -0.1097 0.227 Uiso 0.5 1 calc R U P A -1
C11 C 0.4113(11) 0.0145(14) 0.0425(12) 0.068(5) Uani 0.5 1 d D . P A -1
H11A H 0.3982 -0.0458 0.0758 0.082 Uiso 0.5 1 calc R U P A -1
H11B H 0.3557 0.0267 0.0025 0.082 Uiso 0.5 1 calc R U P A -1
C12 C 0.419(3) 0.097(3) 0.1100(12) 0.074(8) Uani 0.5 1 d D . P A -1
H12A H 0.4554 0.0761 0.1627 0.110 Uiso 0.5 1 calc R U P A -1
H12B H 0.3541 0.1173 0.1285 0.110 Uiso 0.5 1 calc R U P A -1
H12C H 0.4520 0.1521 0.0819 0.110 Uiso 0.5 1 calc R U P A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
I2 Zn1 I1 110.49(5) . .
I2 Zn1 Cl3 108.56(4) . 8_545
I1 Zn1 Cl3 108.38(4) . 8_545
I2 Zn1 I3 108.56(4) . 8_545
I1 Zn1 I3 108.38(4) . 8_545
Cl3 Zn1 I3 0.0 8_545 8_545
I2 Zn1 I3 108.56(4) . .
I1 Zn1 I3 108.38(4) . .
Cl3 Zn1 I3 112.5 8_545 .
I3 Zn1 I3 112.48(6) 8_545 .
C3 N1 C5 111.1(7) . 8_545
C3 N1 C5 111.1(7) . .
C5 N1 C5 107.4(10) 8_545 .
C3 N1 C1 106.1(10) . .
C5 N1 C1 110.6(7) 8_545 .
C5 N1 C1 110.6(7) . .
C7 N2 C7 108.7(4) . 3_565
C7 N2 C7 111.0(8) . 2_665
C7 N2 C7 108.7(4) 3_565 2_665
C7 N2 C7 108.7(4) . 4_655
C7 N2 C7 111.0(8) 3_565 4_655
C7 N2 C7 108.7(4) 2_665 4_655
C9 N3 C11 107.5(12) . .
N1 C1 C2 116.2(14) . .
N1 C1 H1A 108.2 . .
C2 C1 H1A 108.2 . .
N1 C1 H1B 108.2 . .
C2 C1 H1B 108.2 . .
H1A C1 H1B 107.4 . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N1 C3 C4 115.7(12) . .
N1 C3 H3A 108.4 . .
C4 C3 H3A 108.4 . .
N1 C3 H3B 108.4 . .
C4 C3 H3B 108.4 . .
H3A C3 H3B 107.4 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N1 C5 C6 114.4(8) . .
N1 C5 H5A 108.7 . .
C6 C5 H5A 108.7 . .
N1 C5 H5B 108.7 . .
C6 C5 H5B 108.7 . .
H5A C5 H5B 107.6 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N2 C7 C8 113.8(8) . .
N2 C7 H7A 108.8 . .
C8 C7 H7A 108.8 . .
N2 C7 H7B 108.8 . .
C8 C7 H7B 108.8 . .
H7A C7 H7B 107.7 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N3 C9 C10 117(2) . .
N3 C9 H9A 107.9 . .
C10 C9 H9A 107.9 . .
N3 C9 H9B 107.9 . .
C10 C9 H9B 107.9 . .
H9A C9 H9B 107.2 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N3 C11 C12 114.5(18) . .
N3 C11 H11A 108.6 . .
C12 C11 H11A 108.6 . .
N3 C11 H11B 108.6 . .
C12 C11 H11B 108.6 . .
H11A C11 H11B 107.6 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 I2 2.6009(14) .
Zn1 I1 2.6043(15) .
Zn1 Cl3 2.6097(9) 8_545
Zn1 I3 2.6097(9) 8_545
Zn1 I3 2.6098(9) .
N1 C3 1.489(13) .
N1 C5 1.495(10) 8_545
N1 C5 1.495(10) .
N1 C1 1.503(14) .
N2 C7 1.506(9) .
N2 C7 1.506(9) 3_565
N2 C7 1.506(9) 2_665
N2 C7 1.506(9) 4_655
N3 C9 1.481(16) .
N3 C11 1.493(14) .
C1 C2 1.521(18) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2 H2C 0.9700 .
C3 C4 1.494(17) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 H4C 0.9700 .
C5 C6 1.535(13) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 H6C 0.9700 .
C7 C8 1.542(12) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 H8C 0.9700 .
C9 C10 1.52(2) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C10 H10C 0.9700 .
C11 C12 1.52(2) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C12 H12C 0.9700 .
